CN110987612A - Method for evaluating anti-stripping performance of refractory material for silicon deoxidized steel in use process - Google Patents

Method for evaluating anti-stripping performance of refractory material for silicon deoxidized steel in use process Download PDF

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CN110987612A
CN110987612A CN201911073885.7A CN201911073885A CN110987612A CN 110987612 A CN110987612 A CN 110987612A CN 201911073885 A CN201911073885 A CN 201911073885A CN 110987612 A CN110987612 A CN 110987612A
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王昆鹏
徐建飞
谢有
王郢
左锦中
徐和平
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Zenith Steel Group Co Ltd
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Abstract

The invention discloses a method for evaluating the anti-stripping performance of a refractory material for silicon deoxidized steel in a using process, and belongs to the field of ferrous metallurgy. The method is characterized in that: smelting a high-carbon silicon deoxidized steel by using a refractory material to be evaluated, firstly realizing low melting point of endogenous inclusions in the high-carbon silicon deoxidized steel through a refining process, plastically deforming the endogenous inclusions by using a high-temperature rolling process, secondly controlling the final wire rod strength to be more than 1250MPa by controlling a steel rolling process, controlling the diameter of the wire rod to be 10-21mm, immediately sampling and stretching the wire rod after the wire rod is offline, wherein the number of stretched samples is not less than 15, and analyzing and counting fracture ratios caused by inclusions of corundum, magnesia-alumina spinel, zirconia, magnesium-silicon olivine and magnesium oxide by using a scanning electron microscope after stretching. The method can effectively evaluate the anti-stripping performance of the refractory material for the deoxidized steel in the using process.

Description

Method for evaluating anti-stripping performance of refractory material for silicon deoxidized steel in use process
Technical Field
The invention belongs to the field of ferrous metallurgy, and relates to a method for evaluating the anti-stripping performance of a refractory material for silicon deoxidized steel in a using process.
Background
Silicon metal deoxidation is widely used for refining of steel for bead wires, steel for cords, automobile suspension springs, and steel for cutter wires. Researches show that the non-metallic inclusion in the steel can obviously reduce the processing performance and the service performance of the silicon deoxidized steel, and the control of the non-metallic inclusion in the steel is one of the main tasks of steel making. Refractory materials for steel making (including ladle refractory materials, tundish refractory materials, ladle nozzles, stopper rods, submerged nozzles and the like) are one of the main sources of large-size inclusions in steel. The influence mechanism of the refractory material on the cleanliness of molten steel mainly has two modes, one mode is a chemical action which is mainly characterized in that the refractory material and the molten steel or refined slag are subjected to chemical reaction to increase the content of Mg and Al in the molten steel so as to generate or influence nonmetallic inclusions in the steel, the other mode is mainly characterized in that refractory aggregate is peeled off under the scouring action of high temperature and steel flow, and refractory aggregate enters the molten steel in a physical mode. Generally, the size of the inclusions generated under the chemical action is smaller and the harm is smaller, while the size of the inclusions introduced by physical exfoliation is larger and the harm is great. Therefore, the high-temperature anti-stripping performance of the refractory material has great influence on the performance of steel products, and scientific and effective evaluation on the anti-stripping performance of the refractory material can provide important guidance for the selection of the refractory material in the steelmaking process.
However, the distribution of foreign inclusions in the refractory aggregate due to physical exfoliation in the steel is random and accidental, and as for example, only one or a few foreign inclusions due to exfoliation of the refractory aggregate may exist in a wire rod having a length of several meters, and the distribution density in the steel is extremely low, and such inclusions are difficult to detect by a common metallographic or scanning electron microscope method. Therefore, it is difficult to evaluate the spalling resistance of the refractory in the steel making process by the conventional inspection method. For example, in "CN 201710041898.0 method for evaluating inclusions in high aluminum in silicon-killed steel", it solves the problem that the existing method for analyzing inclusions in steel cannot effectively analyze non-plastic inclusions in high aluminum with a size larger than 10um, samples are taken from the process of changing alloy, auxiliary materials or smelting environment significantly, the obtained samples are analyzed by electrolysis and electron microscopy, and then the proportion of inclusions in high aluminum in large-size inclusions is counted by research and analysis. The detection method has extremely high requirements on the operation environment, is low in electrolysis speed and is not suitable for industrial production. In addition, the rotating bending fatigue test is one of the methods for detecting large-sized inclusions in steel. For example, in the research on foreign inclusions in a rotary bending fatigue fracture of silicon deoxidized spring steel 55SiCr, large-size oxide inclusions can be found on the fracture by a rotary bending fatigue test method, but the method has the problems of complicated test process, long test period (weeks or even months) and the like. More importantly, the test method can expose both endogenous and exogenous inclusions on the fracture. When the amount of inclusions in the deoxidized product and the slag inclusion is large and the size is large, it is difficult to find inclusions caused by the flaking of the refractory at the fracture. Therefore, how to quickly and accurately find the foreign inclusions caused by the refractory material in the steel is the key for evaluating the spalling resistance of the refractory material in the using process.
Disclosure of Invention
The invention aims to provide a method for evaluating the anti-stripping performance of a refractory material for silicon deoxidized steel in the using process, aiming at the problem of stripping of the refractory material for silicon deoxidized steel in the using process.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for evaluating the anti-stripping performance of a refractory material for silicon deoxidized steel in the using process is characterized by comprising the following steps:
high carbon silicon deoxidized steel such as 87Mn, 82B and the like is produced using a refractory to be evaluated (including ladle refractory, tundish refractory, ladle nozzle, submerged nozzle and the like), and the spalling resistance of the refractory is evaluated. The process flow comprises the steps of converter/electric furnace-LF refining-continuous casting-rolling-wire rod stretching-fracture inspection and analysis.
① converter/electric furnace procedure, conventional process.
② LF refining process, refining molten steel after tapping in converter/electric furnace, wherein the refining process adopts low-aluminum low-titanium alloy and acid slag refining, and the content of acid-soluble aluminum in steel is controlled within 0.0020%Basicity of refining slag (CaO/SiO)2) Controlling the content of Al in the slag to be 0.8-1.22O3The content is controlled within 10 percent. The refining aims to ensure that both the endogenous inclusion and the coiled slag inclusion in the steel are plastic inclusions and are completely plasticized, thereby avoiding tensile fracture caused by the two types of inclusions and eliminating the interference of the inclusions on fracture.
③ continuous casting and wire rod rolling, wherein the rolling conditions of 87Mn steel include casting blank heating temperature of 1200 + -20 ℃, heating time of 180- & ltSUB & gt 240min, temperature before finish rolling of 840 + -20 ℃, temperature after finish rolling of less than 1020 ℃, temperature before a reducing sizing mill set of 900 + -20 ℃, spinning temperature of 900 + -15 ℃, rolling into wire rods with diameter of 10-21mm, wire rod strength of 1250MPa or above, and conventional controlled rolling and cooling for high carbon silicon deoxidized steel of other materials to make the strength reach 1250MPa or above.
The rolling purpose is three points, one is that the endogenetic inclusion is subjected to full plastic deformation by utilizing high-temperature rolling, the size of the endogenetic inclusion in the width direction is reduced to the maximum extent, and the wire rod fracture caused by the endogenetic inclusion is further reduced or avoided; secondly, the diffusion of carbon atoms is promoted by high-temperature diffusion, and the fracture caused by carbon segregation is reduced; thirdly, the final wire rod is made by controlling the cooling process
Figure BDA0002261783380000021
The strength of the material is controlled to be more than 1250MPa, and the fracture sensitivity of the material to large-size inclusions is increased.
The purpose of the wire rod tensile test is to utilize the stress in the steel and the gas accumulation effect around large-sized inclusions, which are the fracture sources of the material under the condition of stretching, and further expose large-sized inclusions introduced by the spalling of the refractory material in the steel. The method specifically comprises the following steps of carrying out a tensile test on the wire rod after the wire rod is off-line, wherein the time interval between the tensile test and the off-line cannot exceed 8 hours, the diameter of a wire rod is 10-21mm, and not less than 15 drawn samples are obtained.
And collecting fractures, carrying out scanning electron microscope analysis on the fractures, analyzing the sizes and components of inclusions at the fractures, and counting the proportion of the fractures caused by the inclusions consistent with the components of refractory aggregate (alumina, magnesia-alumina spinel, zirconia, magnesia-silica olivine and magnesia).
The key technology of the application is how to lead the material to be just fractured at the inclusion of the refractory material, thereby exposing the inclusion caused by the refractory material.
Compared with the prior art, the invention has the beneficial effects that:
in order to eliminate the interference of the inclusions, the invention controls the inclusions of endogenetic slag and rolling slag into inclusions with low melting point through a refining process, and utilizes a high-temperature diffusion process to plastically deform the inclusions to reduce the size of the inclusions so as to eliminate the interference of the inclusions, so that the inclusions exposed out of a fracture are all foreign inclusions caused by refractory materials. In addition, the method is simple to operate, all the used equipment is common equipment for steel enterprises, other additional equipment is not required, and the test period is short.
In order to expose more of the material-resistant inclusions, the tensile strength of the wire rod needs to be high (>1250MPa), large diameter
Figure BDA0002261783380000031
And the residual stress and residual gas were not allowed to relax (stretching within 8 hours after rolling).
According to the invention, the damage of the inclusions to the material is greatly increased by utilizing the residual stress and the residual gas gathering around the inclusions in the aging period after the high-carbon high-strength steel is rolled, so that the brittle fracture caused by the inclusions in the wire rod stretching process is caused, and the inclusions in the steel are exposed to evaluate the anti-stripping performance of the refractory material. The method can expose the inclusions in the steel on the fracture in a simple mode and determine that the inclusions are all foreign inclusions caused by the refractory material. The spalling property of the refractory material can be evaluated by conventional fracture analysis and inclusion proportion statistics, and effective guidance is provided for the refractory material selection in the silicon deoxidized steel smelting process.
Drawings
FIG. 1 shows tensile fracture morphology caused by inclusions;
FIG. 2 shows the appearance of a fracture caused by corundum as refractory aggregate;
FIG. 3 shows the appearance of a fracture caused by spinel of refractory aggregate;
FIG. 4 shows the appearance of a fracture caused by zirconia as refractory aggregate;
FIG. 5 shows the appearance of a fracture caused by magnesium oxide serving as refractory aggregate;
FIG. 6 shows the appearance of fracture caused by inclusion of slag-type calcium aluminosilicate.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific embodiments:
example 1
Example 1 the refractory was evaluated for spalling resistance of A, B; the refractory A, B is made of alumina-carbon material, but is provided by different manufacturers, and in the using process, except the refractory material, other process parameters and conditions are consistent.
The specific detection method comprises the following steps:
the test steel type is 87Mn, the chemical composition of the test steel type is shown in Table 1, the steel making and rolling process can adopt the cord steel production procedures commonly used in the field, namely converter/electric furnace-LF refining-continuous casting-rolling-wire rod stretching-fracture testing analysis, and the following steps are specifically carried out:
① converter process, wherein the converter end point adopts high carbon-drawing process, proper amount of manganese metal, low-titanium low-aluminum ferrosilicon and carburant are added in the converter tapping process, and the molten steel components are sampled and analyzed rapidly, after tapping, the manganese metal, the low-titanium low-aluminum ferrosilicon and low-melting-point acidic refining slag are added, the addition amount of the manganese metal and the low-titanium low-aluminum ferrosilicon is based on the principle that the content of Mn and Si in steel reaches or approaches to the requirement of finished products, and the addition amount of the low-melting-point acidic refining slag is 8-10 kg/ton steel.
② LF refining process, namely heating the electrode to raise the temperature, adding refining slag to carry out slagging in the tapping process, carrying out bottom argon blowing stirring on a steel ladle in the whole LF treatment process, finely adjusting the components of molten steel to enable the components of the molten steel to meet the requirements of finished products, wherein the total LF treatment time is more than or equal to 45min (the total LF treatment time in example 1 is 47min), and the soft argon blowing time is more than or equal to 25min (the soft argon blowing time in example 1 is 30 min).
LF soft argon blowingAfter the completion of the refining, the basicity (CaO/SiO) of the refining slag is controlled to be less than or equal to 20ppm (the actual measurement value in example 1 is 18ppm) of acid-melted aluminum Als in the molten steel2) The alkalinity is controlled to be 0.8 to 1.2 (the alkalinity is 1.0 in example 1), and Al in the slag2O3The content is controlled within 10% (Al in example 1)2O3Content 9%) dissolved oxygen [ O ]]And at 15-25 ppm, the slag steel fully reacts to ensure that the endogenous inclusions are completely plasticized.
③ continuous casting and wire rod rolling, namely obtaining 160mm x 160mm billet through continuous casting, heating the billet to 1180-.
④ taking 20 wire rods immediately after the wire rods are off line, performing a tensile test, collecting fractures, analyzing the components of fracture inclusions by using a scanning electron microscope, and counting the proportion of the inclusions introduced by physical spalling of the refractory material.
FIG. 1 is a typical inclusion induced tensile fracture with a distinct "white spot" at the fracture; FIGS. 2-5 are typical morphologies of fractures caused by spalling of corundum, spinel, zirconia, and magnesia refractory aggregates, respectively.
Table 2 shows the ratio of fracture due to erosion or spalling of the refractory in example 1, the ratio of fracture due to inclusions in the tensile test piece of the wire rod obtained by using the refractory A is 65%, and the fracture is caused by spalling of the refractory, and the remaining 35% is caused by non-inclusion factors such as abnormal texture, surface damage and the like. And fracture caused by inclusions in the wire rod tensile sample obtained from the refractory material B is caused by the spalling of the refractory material, the fracture proportion is 20 percent, and the rest 80 percent is caused by non-inclusion factors. Therefore, the comparison shows that the stability of the refractory A is lower than that of the refractory B.
By the method, inclusions in steel can be exposed on the fracture, the inclusions can be determined to be all foreign inclusions caused by the refractory material, the exposure of the fracture caused by the spalling of the refractory material due to the influence of the inclusions such as the endogenous inclusions and the rolling slag inclusions is avoided, and therefore the spalling resistance of the refractory material can be evaluated by directly adopting the number of the fractures of the inclusions and the specific gravity of the fracture.
Table 1 test steel grade composition, wt. -%)
C Si Mn P S Cr
0.87-0.90 0.22-0.28 0.82-0.87 <0.010 <0.006 0.20-0.35
TABLE 2 fracture Electron microscopy analysis results
Durable material Total number of tensile specimens Collect the number of fractures, pair Number and proportion of fractures caused by spalling of refractory material
A
20 20 The number of fractures: 13, in a proportion of 65%
B
20 20 The fracture number is 5 percent and accounts for 20 percent
Comparative example 1 20 20 The number of fractures: 0, in proportion of 0%
Comparative example 2 20 20 The number of fractures: 0, in proportion of 0%
Comparative example 1
The refractory a used in comparative example 1 was evaluated for spalling resistance, and the refractory was the same as in example 1.
Comparative example 1 the procedure for evaluating the spalling resistance of the refractory was the same as in example 1, except that the melting point of the inclusions was not reduced in step ②, as compared with example 1.
The specific evaluation method is as follows:
the test steel type is 87Mn, the chemical composition of the test steel type is shown in Table 1, the steel making and rolling process can adopt the cord steel production procedures commonly used in the field, namely converter/electric furnace-LF refining-continuous casting-rolling-wire rod stretching-fracture testing analysis, and the following steps are specifically carried out:
① converter procedure similar to example 1;
② LF refining procedure, the LF refining procedure adopts conventional refining process and the alkalinity (CaO/SiO) of the refining slag2) Controlled at 2.5, Al in slag2O3The content is controlled to be about 25 percent, and acid-soluble aluminum in steel is not controlled intentionally.
③ continuous casting and wire rod rolling procedure similar to example 1;
④ taking 20 wire rods immediately after the wire rods are off line, performing a tensile test, collecting fractures, analyzing the components of fracture inclusions by using a scanning electron microscope, and counting the proportion of the inclusions introduced by physical spalling of the refractory material.
Electron microscopy analysis shows that 20 wire rods have 70% of fracture caused by inclusions, but the components of the inclusions are slag inclusions and are oversized Ca-Al-Si-O inclusions, as shown in FIG. 6. It can be seen that in the comparative example in which the inclusion was not subjected to the low melting point treatment, although the wire breakage ratio caused by the inclusion was increased, the inclusions were all oversized slag inclusions, and the number of inclusion fractures caused by the refractory material was zero, so the spalling resistance of the refractory material could not be evaluated by the number of inclusion fractures and the fracture specific gravity.
Comparative example 2
The refractory a used in comparative example 1 was evaluated for spalling resistance, and the refractory was the same as in example 1.
Comparative example 1 compared with example 1, the evaluation procedure for the spalling resistance of the refractory material is the same as that of example 1, and the main difference is that the final strength of the wire rod in the step ③ is controlled at 1100-1150 MPa.
The specific evaluation method is as follows:
the test steel type is 87Mn, the chemical composition of the test steel type is shown in Table 1, the steel making and rolling process can adopt the cord steel production procedures commonly used in the field, namely converter/electric furnace-LF refining-continuous casting-rolling-wire rod stretching-fracture testing analysis, and the following steps are specifically carried out:
① converter procedure similar to example 1;
② LF refining procedure, same as example 1;
③ continuous casting and wire rod rolling, wherein the strength of the wire rod is controlled within 1100-1150MPa by controlled rolling and controlled cooling;
④ taking 20 wire rods immediately after the wire rods are off line, performing a tensile test, collecting fractures, analyzing the components of fracture inclusions by using a scanning electron microscope, and counting the proportion of the inclusions introduced by physical spalling of the refractory material.
Electron microscope analysis showed that no fracture due to inclusions was observed in 20 wire rods, because when the strength of the wire rod was less than 1200MPa, stress concentration around the inclusions was insufficient to cause breakage of the wire rod, so that the spalling resistance of the refractory material could not be evaluated.
The raw materials and equipment used in the invention are common raw materials and equipment in the field if not specified; the methods used in the present invention are conventional in the art unless otherwise specified. Although the present invention has been described in detail with reference to the above embodiments, it should be understood by those skilled in the art that: modifications and equivalents may be made thereto without departing from the spirit and scope of the invention and it is intended to cover in the claims the invention as defined in the appended claims.

Claims (5)

1. A method for evaluating the anti-stripping performance of a refractory material for silicon deoxidized steel in the using process is characterized by comprising the following steps: the method comprises the steps of smelting high-carbon silicon deoxidized steel by using an aluminum-carbon refractory material to be evaluated, realizing low melting point of endogenous inclusions in the steel through a refining process, controlling the strength of a wire rod to be more than 1250MPa through a high-temperature rolling process, enabling the endogenous inclusions to generate plastic deformation, immediately sampling and stretching the wire rod after the wire rod is taken off line, and finally counting the fracture ratio caused by the inclusions in the refractory material for evaluating the anti-stripping performance of the refractory material for the silicon deoxidized steel in the using process.
2. The method for evaluating the spalling resistance of the refractory material for silicon-killed steel as claimed in claim 1, wherein the operation flow of the evaluation method is as follows: converter-LF refining-continuous casting-rolling-wire rod stretching-fracture inspection and analysis;
wherein in the LF refining process, the content of acid-soluble aluminum in the molten steel is controlled within 0.0020 percent, and the alkalinity (CaO/SiO) of the refining slag is controlled2) Controlling the content of Al in the slag to be 0.8-1.22O3The content is controlled within 10 percent.
3. The method for evaluating the spalling resistance of the refractory for silicon killed steel as set forth in claim 2, wherein said high temperature rolling conditions are: the heating temperature of the casting blank is controlled at 1200 plus or minus 20 ℃, the casting blank is rolled into a wire rod with the diameter of 10-21mm, and the strength of the wire rod is controlled at 1250MPa or above.
4. The method for evaluating the spalling resistance of the refractory for silicon killed steel as set forth in claim 1 or 2, wherein the wire rod is drawn under the conditions: and stretching the wire rod within 8h after the wire rod is off-line.
5. The method for evaluating the spalling resistance of the refractory for silicon deoxidized steel in the using process according to claim 1 or 2, wherein the number of the samples is not less than 15, and the fracture ratio caused by the inclusion of the refractory component is analyzed by using a scanning electron microscope after the stretching.
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CN112525745A (en) * 2020-11-03 2021-03-19 北京科技大学 Physical simulation test device for scouring erosion of tundish lining refractory and using method

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